4-AMINO-5-IODO-2-METHYLBENZONITRILE synthesis

Yield:380241-62-3 66%

Reaction Conditions:

with N-iodo-succinimide;acetic acid at 15 - 20; for 2 h;

Steps:

Step 1: Synthesis of 4-amino-5-iodo-2-methylbenzonitrile

4-Amino-2-methylbenzonitrile (2.64 g, 20 mmol) was dissolved in 30 mL of glacial acetic acid with stirring, The temperature was lowered to 15° C. and NIS (4.5 g, 20 mmol, N-iodosuccinimide) was added in batches, and the reaction was carried out at room temperature for 2 hours after the addition was completed. TLC detected all the disappearance of the raw materials, 60 mL of water was added to the reaction solution, a large amount of white solids were precipitated, stirred for 10 minutes and filtered, The filter cake was washed with 50 mL of water, dried, added with 20 mL of ethyl acetate to make slurry for 1 hour, and filtered to obtain 3.4 g of an off-white solid, yield: 66%. TLC: Rf 0.6 (petroleum ether:ethyl acetate=3:1 by volume).

References:

CN114213396,2022,A Location in patent:Paragraph 0077-0082